Q1: Explain the XRD method to characterize nanomaterials

What is XRD?

• XRD (X-ray Diffraction) is a technique used to study the internal crystal

structure of solid materials.

• It helps us know what the material is made of, how the atoms are arranged, and
whether the structure has any stress or defects.

How does XRD work?

1. A beam of X-rays (with wavelengths ~0.07 to 0.2 nm) is aimed at a crystalline

material.

2. When these X-rays hit the atoms in the crystal, they get diffracted (bent) in
specific directions.

3. This diffraction follows Bragg’s Law:

λ=2dsin⁡θ\lambda = 2d \sin \thetaλ=2dsinθ

o λ = Wavelength of X-rays

o d = Distance between atomic layers (interplanar spacing)

o θ = Angle at which the X-rays are diffracted

4. A detector measures the intensity of the diffracted X-rays at different angles

(2θ).

5. The resulting diffraction pattern (graph) tells us about the material’s structure.

What can XRD tell us?

1. Crystal structure – how atoms are arranged in the solid.

2. Phase identification – what type of material/crystal it is (e.g., quartz, graphite,

etc.).

3. Crystallite size – smaller crystals cause broader peaks.

4. Strain and stress – peak shifts and broadening show if the crystal is under
pressure.

5. Defects – irregularities in the crystal also affect the pattern.

 6. Lattice constants – changes in peak position indicate changes in atomic
spacing.

Special Notes:

• Uniform (homogeneous) strain shifts the peak position.

• Non-uniform (inhomogeneous) strain causes peak broadening.

• Small crystal sizes also lead to broader peaks, which is common in

nanomaterials.

• By analyzing the peak position and shape, we can separate size effects from
strain effects.

Limitations:

• Low sensitivity for materials with light elements (like carbon or oxygen).

• Hard to detect materials that are present in small amounts.

• Works best for crystalline (ordered) materials, not amorphous ones.

XRD Diagram (Explained)

Even if the figure isn’t shown, here’s what a typical XRD setup and pattern look like:

XRD Setup (Layman View)

[X-ray Source] ---> [Sample] ---> (Diffracted X-rays) ---> [Detector rotates at angle 2θ]

X-rays interact with

crystal planes, causing

diffraction at angle θ

• X-rays strike the sample.

• Some of them bounce off (diffract) from the layers of atoms.

• The detector measures the angle and intensity of these diffracted rays.

• This gives a graph of intensity vs 2θ.

XRD Pattern (What it shows)

• A series of peaks appear on a graph.

• Each peak represents a specific atomic spacing.

• The position of the peak = angle (2θ) = tells about distance between layers.

• The height = intensity = tells how strongly the planes diffract the X-rays.

• Width of peak = tells about particle size and strain.

Real-life Use of XRD in Nanomaterials

• Identify types of nanoparticles.

• Measure nanoparticle size (~1–100 nm).

• Analyze stress/strain in nanomaterials like thin films or nanocrystals.

Q2: What is SAXS? Explain SAXS method to characterize materials

What is SAXS (Small Angle X-ray Scattering)?

1. SAXS is a technique that uses X-rays to study the tiny structures inside
materials.

2. It's called “small angle” because it measures how X-rays scatter at very small
angles (0.1° to 10°).

3. It helps scientists see structures between 1 to 100 nanometers, like pores,

particles, or molecular shapes.
How does SAXS work?

1. A thin beam of X-rays is pointed at a sample.

2. Most X-rays pass through, but a few are scattered by the sample.

3. These scattered X-rays hit a detector, forming a pattern.

4. By studying this pattern, scientists can figure out the size, shape, and internal
structure of particles.

What can SAXS tell us?

• Size of particles or pores

• Shape of macromolecules (like proteins)

• How particles are arranged or clustered

• Surface area per volume

• How ordered or disordered the material is

Where is SAXS used?

• Biology: For proteins, DNA, cells, etc. (no need to grow crystals like in XRD)

• Nanotechnology: Nanoparticles, nanocrystals

• Materials science: Plastics, metals, mesoporous materials

• Everyday products: Cement, food, oil, drugs, cosmetics

SAXS Instruments

1. The main parts are an X-ray source, a sample holder, and a detector.

2. SAXS machines block the strong main beam so they can detect the weaker
scattered rays.

3. There are two types of machines:

o Point collimation (more precise)

o Line collimation (faster, less resolution)

 Q3: Difference between XRD and SAXS

SAXS (Small Angle X-ray

Feature XRD (X-ray Diffraction)
Scattering)

Purpose Study crystal structure Study shape, size, and pores

Angle range Wide angles Small angles (0.1° – 10°)

Sample type Needs crystalline material Works on crystalline or amorphous

Information Atomic positions, lattice, Pores, particle size, molecular

given phase structure

Use in biology Needs crystals of proteins Works with liquid proteins

Size range
Atomic scale (0.1 – 1 nm) Nano scale (1 – 100 nm)
studied

Q3: Detailed Difference between XRD and SAXS

SAXS (Small Angle X-ray

Feature XRD (X-ray Diffraction)
Scattering)

XRD is mainly used to determine SAXS is used to study the overall

Purpose the crystal structure of materials. shape, size, surface, and internal
It helps in identifying how atoms pores of nanoparticles or
 SAXS (Small Angle X-ray
Feature XRD (X-ray Diffraction)
Scattering)

are arranged, and whether the molecules — not the exact

material is crystalline or not. atomic positions.

XRD uses wide diffraction angles SAXS uses very small angles (0.1°
(usually >10°) because it looks at to 10°) because it investigates
Angle Range atomic-level spacing between larger structures, like pores or
crystal planes (called interplanar clusters that are much bigger
distance). than atomic layers.

XRD requires the material to be SAXS can be used on both

crystalline (well-ordered atomic crystalline and amorphous
Sample Type structure), or at least partially samples. Even if the sample is a
crystalline. It doesn't work well with gel, liquid, or powder, SAXS can
amorphous (disordered) samples. still give good structural info.

SAXS gives:
XRD gives details like: • Size and shape of particles or
• Atomic arrangement (lattice) pores
Information • Crystal structure & symmetry • Surface-to-volume ratio
Given • Phase identification (e.g., • How particles are grouped
whether it's graphite or diamond) (aggregated)
• Defects and strain in crystals • Density differences inside the
material

SAXS can study proteins in

To study biological samples (like
solution (liquid state) — no need
Use in proteins), XRD needs the protein to
to form crystals. This is super
Biology be crystallized, which is very hard
helpful in biomedical and
and time-consuming.
biochemical research.

SAXS looks at larger structures, in

XRD focuses on very small atomic
the range of 1 – 100 nanometers,
Size Range distances, typically 0.1 – 1
like nanoparticles, pores, or
Studied nanometer (like the distance
clusters — perfect for
between two atoms in a crystal).
nanomaterials.
 Q.4: What is the main difference between a light microscope and an electron
microscope?

Feature Light Microscope Electron Microscope

Source of
Uses visible light Uses a beam of electrons
illumination

Uses electromagnetic or
Uses glass lenses to
Lenses electrostatic lenses to focus
focus light
electrons

Limited to about 200 Much higher — can see objects as

Resolution (ability to
nanometers (can’t see small as 0.1 nanometers (can see
see small details)
viruses, atoms) atoms, nanoparticles)

Magnification Up to 1500x (approx.) Up to 10,00,000x or more

More complex — samples often need

Easier, usually doesn’t
Sample Preparation to be coated, dried, and placed in a
damage the sample
vacuum

Color (natural or stained), Black and white, 2D or 3D depending

Type of image
2D on the type (TEM or SEM)

Simple microscope, TEM (Transmission EM), SEM

Types
Compound microscope (Scanning EM), STEM, etc.

What kind of information can we get from an electron microscope?

Electron microscopes are powerful tools for analyzing nanomaterials, biological

samples, and solid-state materials. Here's what they reveal:

1. Topography (Surface details)

• Shows surface texture – roughness, smoothness, cracks, coatings, etc.

• Helps relate how the surface structure affects material properties like:

o Hardness

o Friction

o Shininess (reflectivity)

2. Morphology (Shape & size)

 • Tells us about the size, shape, and structure of tiny particles or grains.

• Important for understanding properties like:

o Strength

o Ductility (how easily a material bends)

o Reactivity

3. Composition (What it's made of)

• Shows which elements and compounds are present.

• Also tells their relative amounts (e.g., 40% carbon, 30% oxygen).

• Helps relate to properties like:

o Melting point

o Chemical reactivity

o Durability

4. Crystallographic Information (Atomic arrangement)

• Shows how atoms are arranged (crystal structure, defects, grain boundaries).

• Helps us understand:

o Electrical and thermal conductivity

o Mechanical strength

o Magnetic or optical behavior

Basic Working Steps of an Electron Microscope:

1. Electron Gun produces a stream of electrons.

2. Lenses and apertures focus the beam into a thin, sharp beam.

3. Beam is directed at the sample inside a vacuum.

4. When electrons hit the sample, they interact with the atoms.

5. These interactions are detected and used to create a detailed image.

Simple Analogy:
A light microscope is like a flashlight and a magnifying glass — it works fine for big
things like cells.
An electron microscope is like using a laser and ultra-powerful zoom — it lets you
see even the tiny details inside a nanomaterial or a virus.

Q.5: Principle Behind SEM

Basic Principle of SEM (Scanning Electron Microscope):

• SEM works by scanning a focused beam of electrons over the surface of a

sample.

• As the electron beam hits the sample, it interacts with the atoms, producing
signals.

• These signals (especially secondary electrons) are used to create an image of

the surface.

Think of it like:

Instead of shining a flashlight (like in a light microscope), SEM shoots electrons at the
sample and "reads" how they bounce off to map out the surface in super high detail.

Construction of SEM (Main Parts):

1. Electron Gun:

o Produces a stream of electrons.

o These electrons replace light used in normal microscopes.

2. Condenser Lenses (1st & 2nd):

o These focus and narrow the electron beam into a sharp, thin line.

o Condenser aperture helps remove stray, high-angle electrons.

3. Objective Lens & Aperture:

o Final focusing of the beam onto the sample.

o Helps get a clear and high-resolution image.

4. Scanning Coils:

o They move the beam across the sample in a grid or raster pattern (like a
TV screen scanning).
 5. Specimen Chamber:

o Holds the sample in vacuum so that electrons don’t get scattered by air.

o Sample must be solid and properly prepared.

6. Detectors:

o These collect the signals (secondary electrons, backscattered electrons,

X-rays, etc.).

o Signals are converted into an image on the screen.

7. Display System (Monitor/CRT):

o Displays the image pixel by pixel.

o Brightness of each pixel is based on how many electrons were detected.

Working of SEM (Step-by-Step)

1. Electron beam is generated by the electron gun.

2. Beam is focused into a fine spot using condenser and objective lenses.

3. The beam scans over the surface point by point using scanning coils.

4. As the beam hits the sample, it causes emission of:

o Secondary electrons (SE) → Show surface detail

o Backscattered electrons (BSE) → Show contrast based on material

o Characteristic X-rays → Show elemental composition

5. These signals are detected and turned into a real-time image on a monitor.

6. The scanning is so fast that the full image can refresh 30 times per second.

Information SEM Provides

Signal Type What it Tells Us

Secondary Electrons (SE) Surface texture/topography

Backscattered Electrons (BSE) Material contrast/density

X-rays Elemental composition

Signal Type What it Tells Us

Cathodoluminescence (CL) Optical properties

Transmitted Electrons Used in some SEM modes for internal details

Strengths of SEM

• Easy to use for trained users

• Produces high-resolution 3D-like images

• Images can be stored in digital format

• Fast data acquisition for many materials

Limitations of SEM

• Sample must be solid and small enough to fit inside the chamber

• Non-conductive samples (like plastics) need to be coated with a conductive

layer (like gold or carbon)

• Requires vacuum, so wet or soft biological samples need special preparation

Q.6: What is EDS?

EDS = Energy-Dispersive X-ray Spectroscopy

• Also known as:

o EDXA (Energy Dispersive X-ray Analysis)

o EDXMA (Energy Dispersive X-ray Microanalysis)

What it does:

• EDS is used to identify which elements are present in a material and how much
of each element is there.
 • It gives the chemical composition of a sample by analyzing X-rays produced
from it.

Basic Principle of EDS (How it works):

1. An electron beam (usually from an SEM or TEM) hits the sample.

2. The beam knocks out electrons from the inner shells of atoms in the sample.

3. This creates a hole (or vacancy) in the atom’s electron shell.

4. An electron from an outer shell jumps in to fill the hole.

5. The energy difference between the two shells is released as an X-ray.

6. The energy of that X-ray is unique for each element — like a fingerprint.

7. EDS detects these X-rays and tells us what elements are present in the
material.

Why it Works:

• Each element has a unique atomic structure, so it produces a specific X-ray

energy.

• By measuring the energy and number of these X-rays, EDS can identify the
elements and even estimate how much of each element is there.

Main Components of an EDS System:

Component Function

Excitation Usually an electron beam (from SEM or TEM) or X-ray beam (in
Source XRF)

X-ray Detector Detects the X-rays emitted from the sample

Pulse Processor Converts detector signals into readable data

Analyzer Displays and analyzes the elemental spectrum

Where is EDS Used?

• Scanning Electron Microscopes (SEM)

 • Transmission Electron Microscopes (TEM)

• X-ray Fluorescence (XRF) instruments

Types of Detectors:

• Si(Li) Detector: Older, needs liquid nitrogen cooling.

• Silicon Drift Detector (SDD): Newer, uses Peltier cooling (easier to use).

Bonus Concept: Auger Electron

• Sometimes, instead of giving off an X-ray, the atom releases its energy by kicking
out another electron (called an Auger electron).

• This is studied using a different technique called AES (Auger Electron

Spectroscopy).

Summary in Simple Terms:

EDS is like a chemical detective that listens to the X-rays atoms "shout out" when
they’re hit by a beam. Since each atom shouts in its own unique voice (energy level),
EDS can identify them and tell you what your material is made of.
 Q.7: What is the Principle Behind TEM?

Basic Principle of TEM:

• TEM uses a high-energy electron beam that is transmitted (passed through) a

very thin sample.

• When the electrons pass through the sample, they interact with its internal
structure.

• These interactions produce signals (like diffraction, scattering) which are used to
form a high-resolution image of the sample’s internal microstructure.

• The image is then magnified using electromagnetic lenses and displayed on a

screen.

Simple Analogy:

TEM is like shining a flashlight through a thin leaf — the pattern of light that comes
through tells you about the veins and structure inside the leaf.
But instead of light, TEM uses electrons, and it can "see" things much smaller, like
atoms and nanostructures.

Construction of TEM (Main Parts):

1. Electron Gun

o Produces a high-energy stream of electrons.

o Acts like a “light source” in a normal microscope.

2. Condenser Lenses (1 & 2)

o Focus the electron beam into a thin, narrow spot on the sample.

o First lens adjusts spot size, second lens focuses it precisely.

3. Condenser Aperture

o Removes unwanted, high-angle electrons to clean the beam.

4. Sample Holder

o Holds the very thin specimen (a few nanometers thick) in place.

5. Objective Lens

o Focuses the transmitted electrons to form the initial image.

6. Apertures (Optional)
 o Help improve contrast and select specific diffraction areas.

7. Intermediate & Projector Lenses

o Magnify the image further.

8. Fluorescent Screen / CCD Camera

o Converts the electron image into a visible light image.

o Displayed on a monitor or recorded for analysis.

Working of TEM (Step-by-Step):

1. Electron gun shoots a beam of high-speed electrons.

2. Lenses focus the beam into a narrow stream.

3. The beam passes through a very thin sample (must be electron-transparent).

4. Some electrons are absorbed, some are scattered, and some pass through.

5. The transmitted electrons carry information about the internal structure of the
sample.

6. This electron signal is focused and magnified using a series of electromagnetic

lenses.

7. The final image appears on a screen or digital display.

8. Dense areas of the sample appear darker (fewer electrons pass through).

9. Thin or less dense areas appear lighter (more electrons pass through).

Applications of TEM:

• Measure size and shape of individual particles, nanowires, rods, tubes.

• Study internal structure (microstructure) of nanomaterials.

• Determine composition of very small particles.

• Observe defects, crystallinity, and morphology.

• Analyze topography and grain boundaries.

• Helpful in materials science, nanotechnology, and biological research.

 Strengths of TEM:

1. Can see structures as small as 0.1 nm (atomic scale).

2. Excellent for identifying phases, crystal structures, and defects.

3. Ideal for nanomaterials and alloy development.

4. Works well for ultra-thin samples.

Limitations of TEM:

1. Very expensive and large in size.

2. Requires special rooms and maintenance.

3. Needs complex sample preparation (very thin slices).

4. Images are black & white, not colored.

Q.8: Distinguish between XRD, SEM, and TEM

SEM (Scanning
XRD (X-ray TEM (Transmission
S.No Feature Electron
Diffraction) Electron Microscope)
Microscope)

Scanning Electron Transmission Electron

1 Full Form X-ray Diffraction
Microscope Microscope

Based on Bragg's
Based on scattered Based on transmitted
Law: X-rays are
2 Principle electrons from the electrons that pass
diffracted by crystal
surface through the sample
planes

Reveals internal
Identifies crystal Shows surface
structure, grain
3 Purpose structure, phases, features and
boundaries, and
and lattice info composition
crystallography

Bulk structure and Surface morphology Detailed internal

What it
4 average info from and composition of composition of
analyzes
all particles groups of grains individual grains
 SEM (Scanning
XRD (X-ray TEM (Transmission
S.No Feature Electron
Diffraction) Electron Microscope)
Microscope)

Sample Bulk solids or thin Bulk solids or thin Ultrathin samples (<
5
Type/Size films films 100 nm) required

Morphology, surface
Phase, structure, Crystallinity, internal
texture (topology),
6 Main Output lattice parameter, structure, defects, and
elemental
and strain atomic arrangement
composition

Accelerating Not applicable

7 1–30 kV 100–300 kV
Voltage (uses X-rays)

Electron beam Electron beam

8 Wavelength X-rays: ~0.1–0.2 nm wavelength: wavelength:
~nanometers ~picometers

No image; gives
3D-like surface 2D internal image
9 Image Type diffraction pattern
image with atomic resolution
and graphs

Very high (can see

Limited to average
10 Resolution Moderate (a few nm) atoms; < 0.1 nm
atomic distances
resolution)

Structural data Morphology + Atomic structure,

11 Data Type (e.g., crystal Composition (via defects, grain
system) EDS) boundaries, etc.

Phase Surface analysis, Nanomaterials,

identification, material failure defects in crystals,
12 Applications
strain/stress study, industrial biological samples,
analysis materials thin films

Simple Summary:

• XRD → Tells you what material it is and its crystal structure (but not shape or
surface).

• SEM → Tells you the surface features and composition (3D-like images).
 • TEM → Tells you internal atomic structure, crystallinity, and defects in
ultrathin samples.

Q.9: What is STM?

STM = Scanning Tunneling Microscope

• It’s a powerful tool that lets scientists see atoms on a surface.

• Works by measuring the tunneling current between a sharp metal tip and a
conducting surface without touching it.

• Used in nanotechnology and surface science to get atomic-resolution

images.

Principle Behind STM

Quantum Tunneling Effect

• When a sharp metallic tip is brought very close (0.2–1 nm) to a conductive
sample surface, and a small voltage is applied, electrons “tunnel” through the
gap.

• This creates a tunneling current which depends very sensitively on the

distance between tip and surface.

• Even a tiny change in height (less than an atom) causes a large change in current
— this allows detailed mapping of atomic structure.

Construction of STM

Part Function

Sharp metal tip Usually made of tungsten or Pt/Ir, acts as one electrode

Sample holder Holds the conductive surface to be scanned

Piezoelectric
Moves the tip precisely in X, Y, Z directions
scanner

Bias voltage supply Applies a small voltage (10 mV to 1 V) between tip and sample
Part Function

Current detector Measures the tunneling current (0.1 – 10 nA)

Maintains a constant current or height depending on the

Feedback system
mode

Display system Converts movement data into 3D topographic image

Working of STM – Step by Step

1. A bias voltage is applied between the tip and sample.

2. The tip is brought very close to the surface (0.3–1 nm).

3. Electrons tunnel through the tiny gap (due to quantum effect), creating a
tunneling current.

4. As the tip scans over the surface, the tunneling current is measured.

5. Either the current is kept constant (by moving the tip up/down) or height is kept
constant (current varies).

6. The position of the tip is recorded to create an atomic-resolution image of the

surface.

Positive and Negative Bias:

Bias Type Direction of Electron Flow What Happens

Negative bias (sample is Electrons flow from Electrons tunnel out of the
negative) sample → tip sample

Positive bias (sample is Electrons flow from tip → Electrons tunnel into the
positive) sample sample

• Direction of current flow changes based on bias polarity.

• This affects which electronic states are imaged (occupied or unoccupied).

Modes of Operation of STM

1⃣ Constant Current Mode

 • Tunneling current is kept constant.

• Feedback adjusts the height of the tip as it scans.

• Tip moves up and down to follow the surface atoms.

• Gives high contrast and detailed topography.

• Slower scan but more accurate.

2⃣ Constant Height Mode

• Tip height is kept constant, and current is measured as it changes.

• Useful for flat surfaces.

• Faster scanning, but less contrast on rough surfaces.

• Current variations indicate surface features.

STM Resolution

• X, Y resolution (horizontal): ~0.01 nm

• Z resolution (vertical): ~0.002 nm

• That means STM can see individual atoms and map 3D surface structures!

Summary

Aspect STM Description

Technique Scans a sharp tip over a surface to measure electron tunneling

Works on Conductive samples only

Tip-Sample
~0.3–1 nm
Distance

Key Effect Quantum tunneling

Bias Voltage 10 mV to 1 V

Current Range 0.1 to 10 nA

Resolution Atomic-scale (0.01 nm lateral, 0.002 nm vertical)

Aspect STM Description

Modes Constant Current and Constant Height

Imaging atoms, nanostructures, surface defects, electron

Applications
density